CN109437205A - A kind of monocrystalline high-purity carborundum and preparation method thereof - Google Patents
A kind of monocrystalline high-purity carborundum and preparation method thereof Download PDFInfo
- Publication number
- CN109437205A CN109437205A CN201811586340.1A CN201811586340A CN109437205A CN 109437205 A CN109437205 A CN 109437205A CN 201811586340 A CN201811586340 A CN 201811586340A CN 109437205 A CN109437205 A CN 109437205A
- Authority
- CN
- China
- Prior art keywords
- preparation
- purity
- monocrystalline
- silicon carbide
- purity carborundum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of monocrystalline high-purity carborundums and preparation method thereof, design silicon carbide preparation technical field, comprising the following steps: step 1), treatment of silica: step 2), particle purification: step 3), crystallization.Present invention process is simple and practical, and there is environment protecting, impurity-eliminating effect can be played by alkali cleaning and pickling process, effectively reduce the impurity such as silicate in single-crystal silicon carbide, its purity can be made to reach 99% or more, 95% compared with traditional approach totally exceeds 0.5 percentage point, improve the core competitiveness of company, in addition it is effectively increased the heating conduction of product, antioxidant effect can be played at high temperature, silicon carbide addition sawdust and sodium chloride when smelting crystallization, sodium chloride can carry out the impurity such as iron aluminium in silicon-carbide particles further removing to improve whole purity, sawdust can play the carbon monoxide for excluding to generate when smelting, carbon monoxide is avoided to damage working region and natural environment.
Description
Technical field
The present invention relates to silicon carbide preparation technical field, specifically a kind of monocrystalline high-purity carborundum and preparation method thereof.
Background technique
Diamond dust also known as silicon carbide are to pass through the smelting of resistance furnace high temperature with raw materials such as quartz sand, petroleum coke (or coal tar), sawdusts
It refines, there is also rare mineral in the Nature for silicon carbide, and Mo Sangshi, silicon carbide is also known as moissanite, non-in contemporary C, N, B etc.
In oxide high-tech refractory raw material, silicon carbide is most widely used, most economical one kind, is properly termed as corundum or fire resisting
Sand, silicon carbide due to stable chemical performance, thermal coefficient is high, thermal expansion coefficient is small, wear-resisting property is good, except making abrasive material with outer, and also
There are a lot of other purposes.
The growing method for the single-crystal silicon carbide being currently known mainly has sublimed method, Acheson's method, and sublimed method is that growth SiC is mono-
Brilliant one of most popular method, is using SiC as raw material, and being heated makes its distillation, makes the method for monocrystalline precipitation in low temperature portion, this
Kind method is related to the Various Complexes process such as thermodynamics, dynamics and mass transfer and heat transfer, in crystal growing process
There are multiple parameters to need to optimize, and since the partial pressure for being difficult to be formed gas after raw material distils controls as the group in stoichiometry
At, thus cause often to exist in prepared monocrystalline dislocation, micro-pipe, low-angle boundary, cavity are posted polytype etc. and are fallen into, thus shadow
The quality of crystal obtained by ringing, Acheson's method is to make the method for carbon and alkali silica reaction at high temperature, and this method is deposited in the feed
In a large amount of impurity, it is difficult to improve purity, but also the more difficult large-sized crystal of acquisition.Therefore, those skilled in the art provide
A kind of monocrystalline high-purity carborundum and preparation method thereof, to solve the problems mentioned in the above background technology.
Summary of the invention
The purpose of the present invention is to provide a kind of monocrystalline high-purity carborundums and preparation method thereof, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the invention provides the following technical scheme: a kind of monocrystalline high-purity carborundum and its preparation side
Method, comprising the following steps:
Step 1), treatment of silica:
S1, silica is subjected to break process through air-flow powder milling crusher machine, while by vibrating screen to broken micro-
Grain is screened；
S2, the particle after screening is put into magnetic separator the magnetic material that it contains is completely separated；
Step 2), particle purification:
A1, it the particle after magnetic separation is put into reaction kettle while being added water and kerosene is stirred at normal temperature, stirring is extremely
Until slurry foaming floats free charcoal, it is floating to skim free charcoal；
A2, deionized water and sodium hydroxide progress alkali cleaning are added into reaction kettle, while reaction kettle inner space being heated
It to 80 DEG C, is stood after persistently stirring 6 hours, time of repose was controlled at 10 hours；
A3, pour out lye, while heating pickling solution, at the same 80 DEG C at a temperature of stirring 6 hours after stand, time of repose
Control at 5 hours, be added deionized water after through stir filters pressing, repeatedly 3-4 times until PH reaches 7；
A4, the slurry after pickling is put into waterpower overflow cylinder, sodium silicate dispersion is added, control flow divides it
Grade, the particle after classification is by drying, the silicon powder after being purified.
Step 3), crystallization:
B1, silicon powder is fitted into vertical electric arc furnaces, while furnace burdening is added；
B2, energization make furnace temperature rise to 2600-2700 DEG C, and constant temperature is smelted 25-50 hours, utilize the height generated inside electric arc furnaces
Warm high pressure makes silicon-carbide particles by recrystallizing；
High-purity carborundum monocrystalline is obtained after B3, power-off, after natural cooling.
As a further solution of the present invention: the aperture of vibrating screen mesh is 30-50 mesh in step 1).
As a further solution of the present invention: deionized water and sodium hydroxide press the ratio of silicon carbide micro-powder in the step 2)
Example is 1:5:0.015, while the ratio of silicon carbide micro-powder and water and kerosene is 1:1:0.001.
As a further solution of the present invention: the pickling solution in the step 2) is mixed by water, the concentrated sulfuric acid and hydrofluoric acid
It forms, wherein the concentration of the concentrated sulfuric acid is 98%, the concentration of hydrofluoric acid is 45%, and silicon carbide micro-powder, water, the concentrated sulfuric acid, hydrogen fluorine
The ratio of acid is 1:0.7:0.3:0.002.
As a further solution of the present invention: the drying in the step 2) is dried using flash evaporation drying equipment, into
Draught temperature is 250 DEG C, 120 ° of discharge port temperature.
As a further solution of the present invention: the power of the vertical electric arc furnaces of the step 3) is 7000KVA, and its furnace
The size of thorax is φ 3m × 2.5m.
As a further solution of the present invention: pre-buried two graphite electrodes, furnace core body in the burner hearth of the vertical electric arc furnaces
It is connected between two electrodes, and graphite electrode use allows to be greater than 25A/cm2 using current density.
As a further solution of the present invention: the furnace burdening in the step 3) includes quartz, coke, sawdust and chlorination
Sodium.
Compared with prior art, the beneficial effects of the present invention are: present invention process is simple and practical, and there is environment protecting,
Impurity-eliminating effect can be played by alkali cleaning and pickling process, the impurity such as silicate in single-crystal silicon carbide is effectively reduced, it can be made
Purity reaches 99% or more, and 95% compared with traditional approach totally exceeds 0.5 percentage point, is in addition effectively increased leading for product
Hot property, can play antioxidant effect at high temperature, silicon carbide addition sawdust and sodium chloride when smelting crystallization, and sodium chloride can be with
The impurity such as iron aluminium in silicon-carbide particles further remove to improve whole purity, sawdust can the row of playing when smelting
Except the carbon monoxide of generation, carbon monoxide is avoided to damage working region and natural environment, optimize working environment, solved
Carbon monoxide of having determined sucking human body be easy to cause different degrees of the problem of endangering.
Detailed description of the invention
Fig. 1 is a kind of process frame diagram of monocrystalline high-purity carborundum and preparation method thereof.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, in the embodiment of the present invention, a kind of monocrystalline high-purity carborundum and preparation method thereof, including following step
It is rapid:
Step 1), treatment of silica:
S1, silica is subjected to break process through air-flow powder milling crusher machine, while by vibrating screen to broken micro-
Grain is screened；
S2, the particle after screening is put into magnetic separator the magnetic material that it contains is completely separated, impurity elimination can be played
Effect, guarantee the quality and purity of particle；
Step 2), particle purification:
A1, it the particle after magnetic separation is put into reaction kettle while being added water and kerosene is stirred at normal temperature, stirring is extremely
Until slurry foaming floats free charcoal, it is floating to skim free charcoal；
A2, deionized water and sodium hydroxide progress alkali cleaning are added into reaction kettle, while reaction kettle inner space being heated
It to 80 DEG C, is stood after persistently stirring 6 hours, time of repose was controlled at 10 hours；
A3, pour out lye, while heating pickling solution, at the same 80 DEG C at a temperature of stirring 6 hours after stand, time of repose
Control at 5 hours, be added deionized water after through stir filters pressing, repeatedly 3-4 times until PH reaches 7；
A4, the slurry after pickling is put into waterpower overflow cylinder, sodium silicate dispersion is added, control flow divides it
Grade, the particle after classification is by drying, the silicon powder after being purified.
Step 3), crystallization:
B1, silicon powder is fitted into vertical electric arc furnaces, while furnace burdening is added；
B2, energization make furnace temperature rise to 2600-2700 DEG C, and constant temperature is smelted 25-50 hours, utilize the height generated inside electric arc furnaces
Warm high pressure makes silicon-carbide particles by recrystallizing；
High-purity carborundum monocrystalline is obtained after B3, power-off, after natural cooling.
The aperture of vibrating screen mesh is 30-50 mesh in step 1).
Deionized water and sodium hydroxide are 1:5:0.015 in the ratio of silicon carbide micro-powder in step 2), while silicon carbide is micro-
The ratio of powder and water and kerosene is 1:1:0.001.
Pickling solution in step 2) is mixed by water, the concentrated sulfuric acid and hydrofluoric acid, wherein the concentration of the concentrated sulfuric acid be 98%,
The concentration of hydrofluoric acid is 45%, and the ratio of silicon carbide micro-powder, water, the concentrated sulfuric acid, hydrofluoric acid is 1:0.7:0.3:0.002.
Drying in step 2) is dried using flash evaporation drying equipment, and intake air temperature is 250 DEG C, discharge port temperature
120°。
The power of the vertical electric arc furnaces of step 3) is 7000KVA, and the size of its burner hearth is φ 3m × 2.5m.
Pre-buried two graphite electrodes in the burner hearth of vertical electric arc furnaces, furnace core body is connected between two electrodes, and graphite
Electrode, which uses, to be allowed to be greater than 25A/cm2 using current density.
Furnace burdening in step 3) includes quartz, coke, sawdust and sodium chloride.
Impurity-eliminating effect can be played by alkali cleaning and pickling process in summary, effectively reduce silicic acid in single-crystal silicon carbide
The impurity such as salt can make its purity reach 99% or more, and 95% compared with traditional approach totally exceeds 0.5 percentage point, in addition effectively
The heating conduction for increasing product, can play antioxidant effect at high temperature, silicon carbide when smelting crystallization addition sawdust and
Sodium chloride, sodium chloride can carry out the impurity such as iron aluminium in silicon-carbide particles further removing to improve whole purity, sawdust
The carbon monoxide for excluding to generate can be played when smelting, and carbon monoxide is avoided to cause brokenly working region and natural environment
It is bad, working environment is optimized, solves the problems, such as that carbon monoxide sucking human body be easy to cause different degrees of endanger.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of monocrystalline high-purity carborundum and preparation method thereof, which comprises the following steps:
Step 1), treatment of silica:
S1, by silica through air-flow powder milling crusher machine carry out break process, while by vibrating screen to broken particle into
Row screening；
S2, the particle after screening is put into magnetic separator the magnetic material that it contains is completely separated；
Step 2), particle purification:
A1, it the particle after magnetic separation is put into reaction kettle while being added water and kerosene is stirred at normal temperature, stirring to slurry
Until foaming floats free charcoal, it is floating to skim free charcoal；
A2, deionized water and sodium hydroxide progress alkali cleaning are added into reaction kettle, while reaction kettle inner space is heated to 80
DEG C, it is stood after persistently stirring 6 hours, time of repose was controlled at 10 hours；
A3, pour out lye, while heating pickling solution, at the same 80 DEG C at a temperature of stirring 6 hours after stand, time of repose control
At 5 hours, be added deionized water after through stir filters pressing, repeatedly 3-4 times until PH reaches 7；
A4, the slurry after pickling being put into waterpower overflow cylinder, sodium silicate dispersion is added, control flow is classified it, point
Particle after grade is by drying, the silicon powder after being purified.
Step 3), crystallization:
B1, silicon powder is fitted into vertical electric arc furnaces, while furnace burdening is added；
B2, energization make furnace temperature rise to 2600-2700 DEG C, and constant temperature is smelted 25-50 hours, high using the high temperature generated inside electric arc furnaces
Pressure makes silicon-carbide particles by recrystallizing；
High-purity carborundum monocrystalline is obtained after B3, power-off, after natural cooling.
2. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
1) aperture of vibrating screen mesh is 30-50 mesh in.
3. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
2) deionized water and sodium hydroxide are 1:5:0.015 in the ratio of silicon carbide micro-powder in, while silicon carbide micro-powder and water and kerosene
Ratio be 1:1:0.001.
4. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
2) pickling solution in is mixed by water, the concentrated sulfuric acid and hydrofluoric acid, and wherein the concentration of the concentrated sulfuric acid is the concentration of 98%, hydrofluoric acid
It is 45%, and the ratio of silicon carbide micro-powder, water, the concentrated sulfuric acid, hydrofluoric acid is 1:0.7:0.3:0.002.
5. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
2) drying in is dried using flash evaporation drying equipment, and intake air temperature is 250 DEG C, 120 ° of discharge port temperature.
6. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
3) power of vertical electric arc furnaces is 7000KVA, and the size of its burner hearth is φ 3m × 2.5m.
7. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that described vertical
Pre-buried two graphite electrodes, furnace core body are connected between two electrodes in the burner hearth of electric arc furnaces, and graphite electrode is using permission
It is greater than 25A/cm2 using current density.
8. a kind of monocrystalline high-purity carborundum according to claim 1 and preparation method thereof, which is characterized in that the step
3) furnace burdening in includes quartz, coke, sawdust and sodium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811586340.1A CN109437205A (en) | 2018-12-25 | 2018-12-25 | A kind of monocrystalline high-purity carborundum and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811586340.1A CN109437205A (en) | 2018-12-25 | 2018-12-25 | A kind of monocrystalline high-purity carborundum and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109437205A true CN109437205A (en) | 2019-03-08 |
Family
ID=65535149
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811586340.1A Pending CN109437205A (en) | 2018-12-25 | 2018-12-25 | A kind of monocrystalline high-purity carborundum and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109437205A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
| CN110818425A (en) * | 2019-12-06 | 2020-02-21 | 江西拓普准晶新材料股份有限公司 | Method for processing silicon carbide recrystallization sintering high-purity ceramic abrasive by using powdered quartz |
| CN115012028A (en) * | 2022-07-01 | 2022-09-06 | 山西中电科新能源技术有限公司 | Method for preparing large-size silicon carbide crystals |
| CN116750772A (en) * | 2023-08-18 | 2023-09-15 | 江苏中腾石英材料科技股份有限公司 | Silicon micropowder purification device |
-
2018
- 2018-12-25 CN CN201811586340.1A patent/CN109437205A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
| CN110818425A (en) * | 2019-12-06 | 2020-02-21 | 江西拓普准晶新材料股份有限公司 | Method for processing silicon carbide recrystallization sintering high-purity ceramic abrasive by using powdered quartz |
| CN115012028A (en) * | 2022-07-01 | 2022-09-06 | 山西中电科新能源技术有限公司 | Method for preparing large-size silicon carbide crystals |
| CN116750772A (en) * | 2023-08-18 | 2023-09-15 | 江苏中腾石英材料科技股份有限公司 | Silicon micropowder purification device |
| CN116750772B (en) * | 2023-08-18 | 2023-11-28 | 江苏中腾石英材料科技股份有限公司 | Silicon micropowder purification device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109437205A (en) | A kind of monocrystalline high-purity carborundum and preparation method thereof | |
| CN109502589A (en) | A method of preparing high-purity silicon carbide powder | |
| CN103508454B (en) | A kind of preparation method of high-purity silicon carbide raw material | |
| JP4856738B2 (en) | Manufacturing method of high purity silicon material | |
| CN107935007B (en) | Method for preparing high-temperature low-sodium alumina by secondary roasting | |
| FR2918999A1 (en) | PROCESS FOR MANUFACTURING SOLAR QUALITY POLYSILICON INGOTS WITH APPROPRIATE INDUCTION APPARATUS | |
| WO2011150771A1 (en) | Method for producing bauxite-based hollow corundum sphere | |
| US20120171848A1 (en) | Method and System for Manufacturing Silicon and Silicon Carbide | |
| CN105883780A (en) | Method for preparing high-purity flake graphite | |
| JP2018016498A (en) | Method for manufacturing silicon carbide single crystal ingot | |
| CN107758670A (en) | A kind of preparation method of boron carbide superfine powder | |
| CN109320216A (en) | A kind of calcium hexaluminate crucible manufacturing modified based on laminar structured rare earth oxide | |
| JPS61117111A (en) | Manufacture of metal silicon for light-generating-electric industry | |
| CN111777417A (en) | Silicon carbide-carbon ramming mass for blast furnace slag high-temperature carbonization electric furnace and preparation method thereof | |
| CN108301041A (en) | A kind of crucible used for polycrystalline silicon ingot casting and preparation method thereof | |
| CN111039322A (en) | Preparation method of high-activity zirconia | |
| CN107954718A (en) | A kind of preparation method of boron carbide smelting device and boron carbide | |
| CN107244930A (en) | A kind of resistance to molten iron corrodes blast furnace carbon brick and preparation method thereof | |
| CN103979981A (en) | A large-size semi-graphite silicon carbide carbon brick and a production process thereof | |
| CN206562476U (en) | A kind of silicon melting furnaces for lifting silicon material fritting efficiency | |
| CN105777128A (en) | Method for synthesizing hafnium carbide ceramic powder at low temperature through assisting of molten salts and magnesiothermic reduction | |
| CN104016316A (en) | Method for continuously preparing aluminum nitride powder and equipment thereof | |
| CN103757703B (en) | A kind of High-purity large-size silicon carbide single crystal and preparation technology thereof | |
| CN107557863B (en) | Production method of monocrystal electric melting alumina | |
| WO2020057095A1 (en) | Method for preparing silicon carbide powder by using induction furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190308 |